Dataset : Boosting 1H and 13C NMR signals by orders of magnitude on a bench
Description
Spectroscopic Data DNP 1T 77K
1H DNP Juice with TEMPOL at 50mM
Sample : 6/2/2 DMSO-d6/H2O/D2O 200µL
Topspin Folder : 20231102_HDNPjuice_50mM_CB
Note : no phc1 in the data processing not to affect the integral as we have a broad signal
- TE : 100 / 200 / 300
- substraction of the 100 TE and 1000 BG with Topspin —> exp 1
- For 200 w BG1000 —> exp 2 proc 999
- For 300 w BG1000 —> exp 3 proc 999
- DNP : 105 / 205 / 305
- MW 28,16 GHz ± 20 MHz @ 60 kHz
- E 105 (comp to 2) : 110
- E 205 (comp to 3) : 97
- E 305 (comp to 4) : 95
- T build up with satrec : 206
- 28,18 GHz no fmod
General model:
val(t) = a*(1-exp(-(t)/T)+d)
Coefficients (with 95% confidence bounds):
T = 0.5164 (0.4523, 0.5805)
a = 0.7312 (0.6996, 0.7628)
d = 0.3518 (0.3163, 0.3873)
- T1 : 207
- satrec experiment at TE
- General model:
- val(t) = a*(1-exp(-(t)/T)+d)
- Coefficients (with 95% confidence bounds):
- T = 0.5067 (0.4584, 0.555)
- a = 0.7826 (0.7567, 0.8085)
- d = 0.2713 (0.2458, 0.2967)
Notes
1H HYPSO NL-104A at 43 µmol/cm3 of TEMPOL
Sample : 8/2 D2O/H2O 46,4µL impregnated in 73,7 mg HYPSO
Topspin Folder : 20231116_1H_HYPSO_43
- TE : 10
- for quantification (proc 997 of exp1) : subtracted from background 1000 (with lb 1000Hz)
- for plot 10 (proc 998 exp 1 phased 0)
- DNP : 105
- MW 28,17 GHz ± 20 MHz with frequency modulation @ 60kHz
- E = 62 (comp to proc 997 and with lb 1000 Hz)
- T build up with satrec : 106
- T1 : 107
- satrec experiment at TE
- General model:
val(t) = a*(1-exp(-(t)/T)+d)
Coefficients (with 95% confidence bounds):
T = 0.8797 (0.6137, 1.146) ± 0,27
a = 0.828 (0.7287, 0.9273)
d = 0.208 (0.1427, 0.2732)
Notes
13C HYPSO NL-104A at 43 µmol/cm3 of TEMPOL
Sample : 8/2 D2O/H2O + 3.00M acetate 42 µL impregnated in 66.6 mg of HYPSO
Topspin Folder : 20240205_13C_Acetate
- CP-DNP :
- without flipback 405 at 28,35 GHz
- T CP build up :
- General model:
- val(t) = a*(1-exp(-(t)/T)+d)
- Coefficients (with 95% confidence bounds):
- T = 0.8274 (0.7077, 0.9471)
- a = 0.9999 (0.9465, 1.053)
- d = -0.004187 (-0.03447, 0.0261)
- with 403 MW 28,32 GHz w freq mod
- with satrec, flipback and echo
- from -2280 to -2550 ppm
- General model:
- 13C DNP buildup / T1 : 408
- delay incremented after CP
- delay from until 60 s
- at 28,35 GHz w freq mod
- From 6592 to 6360 ppm
General model:
val(t) = a*(exp(-(t)/T)+d)
Coefficients (with 95% confidence bounds):
T = 18.26 (16.55, 19.98)
a = 1.008 (0.9698, 1.046)
d = -0.01884 (-0.05639, 0.0187)
Notes
13C DNP Juice with TEMPOL at 50mM
Sample : 6/2/2 DMSO-d6/H2O/D2O + 3M Sodium Acetate and 50mM TEMPOL
Topspin folder : 20240205_13C_Acetate and 20240122_13C_HYPSO_2 (for CP build up)
Data folder path :
- Direct 13C DNP : 301
- MW 28,17 GHz w freq mod
- without echo is 300
- CP-DNP :
- without flipback 205 (8NS) @ 28,15 GHz —> E = comp to 209
- Direct 13C DNP T build up : 305
- using satrec under DNP until 50 s
- 12 s
- at 28,22 GHz w freq mod
- from -2800 ppm. to -3050 ppm
General model:
val(t) = a*(1-exp(-(t)/T)+d)
Coefficients (with 95% confidence bounds):
T = 12.18 (10.43, 13.94)
a = 1.083 (1.02, 1.147)
d = -0.04458 (-0.07104, -0.01813)
- T1 13C : 211
- delay incremented after CP
- delay from until 50 s
- at 28,22 GHz w freq mod
- From 5880 to 5620 ppm
General model:
val(t) = a*(exp(-(t)/T)+d)
Coefficients (with 95% confidence bounds):
T = 12.03 (10.3, 13.76)
a = 1.399 (1.318, 1.481)
d = -0.284 (-0.3274, -0.2406)
- CP DNP build up : 202 (wit DNP juice !! wrong title. But wrong sample positioning this day)
- MW 28,16 GHz w freq mod
- from -8660 to -8900 ppm
General model:
val(t) = a*(1-exp(-(t)/T)+d)
Coefficients (with 95% confidence bounds):
T = 0.6656 (0.6019, 0.7294)
a = 0.9957 (0.962, 1.029)
d = -0.01011 (-0.03077, 0.01056)
Files
Data_Zenodo.zip
Files
(14.4 MB)
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